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新型联萘酚杂化介孔硅胶的制备及其性能研究

杨漾, 钱洁, 李莉, 狄斌

杨漾, 钱洁, 李莉, 狄斌. 新型联萘酚杂化介孔硅胶的制备及其性能研究[J]. 中国药科大学学报, 2014, 45(5): 557-562. DOI: 10.11665/j.issn.1000-5048.20140509
引用本文: 杨漾, 钱洁, 李莉, 狄斌. 新型联萘酚杂化介孔硅胶的制备及其性能研究[J]. 中国药科大学学报, 2014, 45(5): 557-562. DOI: 10.11665/j.issn.1000-5048.20140509
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YANG Yang, QIAN Jie, LI Li, DI Bin. Preparation and characterization of a novel HPLC stationary phase binaphthyl functionalized mesoporous silica[J]. Journal of China Pharmaceutical University, 2014, 45(5): 557-562. DOI: 10.11665/j.issn.1000-5048.20140509
Citation: YANG Yang, QIAN Jie, LI Li, DI Bin. Preparation and characterization of a novel HPLC stationary phase binaphthyl functionalized mesoporous silica[J]. Journal of China Pharmaceutical University, 2014, 45(5): 557-562. DOI: 10.11665/j.issn.1000-5048.20140509
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新型联萘酚杂化介孔硅胶的制备及其性能研究

  • 1.

    中国药科大学药物分析教研室

  • 2.

    新疆医科大学药学院

  • 3.

    中国药科大学药物质量与安全预警教育部重点实验室

基金项目: 新疆维吾尔族自治区自然科学基金资助项目(No.201233146-7)

Preparation and characterization of a novel HPLC stationary phase binaphthyl functionalized mesoporous silica

摘要

    摘要
  • 摘要: 利用3-异氰基丙基三乙氧基硅烷(ICPTES)与联萘二酚合成联萘酚单硅酯，首次在酸性条件下利用联萘酚单硅酯与1，2-三乙氧基硅基乙烷(BTSE)作为共同硅源，以阳离子表面活性剂十六烷基三甲基溴化铵(CTAB)和聚环氧乙烷-聚环氧丙烷-聚环氧乙烷三嵌段共聚物P123为共模板剂，合成出粒径3~5 μm，平均孔径约5 nm的新型联萘酚杂化介孔硅胶。应用于联萘类衍生物的分离研究，结果显示该固定相机械强度较好，在15 min内对5种联萘类衍生物能够达到基线分离，并且对联萘类衍生物的分离性能优于商品化硅胶柱。
    Abstract: In this study, a novel silica source named M-bionl was synthesized by(3-isocyanatopropyl)-triethoxysilane(ICPTES)and R-(+)-1, 1′-bi-2-naphthol. A new mesoporous silica was first obtained by M-bionl and Bis(triethoxysilyl)ethane(BTSE)as co-silica source, hexadecyl trimethyl ammonium bromide(CTAB)and PEO-PPO-PEO(P123)as co-template in acid condition. The diameter of particles was 3-5 μm with mean pore size of 5 nm. Then the separation capacity of the mesoporous silicas was tested, with excellent mechanical strength and complete separation of 5 kinds of binaphthyl compounds being achieved within 15 min, which indicated a promising application of these mesoporous silicas in HPLC and their separation performance was superior to commercial silica for binaphyhyl compounds.
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    • 参考文献(11)
  • [1] Frank H,Maxinilian C,Jurgen M,et al.Silica-based mesoporous organic-inorganic hybrid materials[J].Angew Chem Int Ed,2006, 45(20):3 216-3 251.
    [2] Yokoi T,Kubota Y,Tatsumi T.Amino-functionalized mesoporous silica as base catalyst and adsorbent[J].Appl Catal A,2012,421/422:14-37.
    [3] Guan LY,Di B,Su MX,et al.Immoblization of β-glucosidase on bifunctional periodic mesoporous organosilicas[J].Biotechnol Lett,2013,35(8):1 323-1 330.
    [4] Sheng LL,Chen JL,Su MX,et al.Synthesis and characterization of folic acid modified mesoporous silica nanoparticles and its loading performance of realgar[J].J China Pharm Univ(中国药科大学学报),2014,45(3):314-319.
    [5] Li C, Di B, Hao WQ, et al. Preparation and chromatographic application of novel periodic mesoporous organosilicas[J].J China Pharm Univ(中国药科大学学报),2012,41(2):151-155.
    [6] Moreau JJE, Vellutini L, Man MWC, et al. Shape-Controlled bridged silsesquioxanes:hollow tubes and spheres[J].Chem Eur J,2003,9(7):1 594-1 599.
    [7] Ran RX,Di B,Chang JM.Synthesis and characteraziton of C8-functionalized ordered mesoporous aminopropyl-silica[J].J Xinjiang Med Univ(新疆医科大学学报),2012,35(3):315-318.
    [8] Huang LL, Lu J, Di B, et al. Self-assembled highly ordered ethanebridged periodic mesoporous organosilica and its application in HPLC[J].J Sep Sci,2011,34(18):2 523-2 527.
    [9] Lu J, Huang LL, Di B, et al. Spherical periodic mesoporous organosilicas bearing camphorsulfonamide substructures for HPLC[J].Chromatographia,2011,74(7):515-521.
    [10] Wang PY,Yang J,Liu J,et al.Chiral mesoporous organosilicas with R-(+)-Binol integrated in the framework[J].Microporous Mesoporous Mater,2009,117(1/2):91-97.
    [11] Ran RX,You LJ,Di B,et al.A novel chiral mesoporous binaphthyl-silicas:preparation,characterization,and application in HPLC[J].Sep Sci,2012,35(15):1 854-1862.
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  • 刊出日期:  2014-10-24

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